CN103050671A - Preparation method of tin carbon composition material for lithium ion battery negative pole - Google Patents
Preparation method of tin carbon composition material for lithium ion battery negative pole Download PDFInfo
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- CN103050671A CN103050671A CN2012105049443A CN201210504944A CN103050671A CN 103050671 A CN103050671 A CN 103050671A CN 2012105049443 A CN2012105049443 A CN 2012105049443A CN 201210504944 A CN201210504944 A CN 201210504944A CN 103050671 A CN103050671 A CN 103050671A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a tin carbon composition material for a lithium ion battery negative pole. The method comprises the following steps of: (1) fully dissolving synthetic resin in an alcohol solvent; (2) firstly adding tin salt in a solution under the function of stirring and ultrasonic, adding graphite in the solution after stirring for 3-8 hours, and stirring for 2-5 hours; (3) dropwise adding ammonia water in the solution until the pH value of the system is 8; (4) carrying out vacuum drying on the system under 130-140 DEG C, and keeping 4-6 hours; and (5) carrying out mechanical ball milling on products, raising the temperature to 900-1100 DEG C, and keeping for 2-5 hours in an inert gas atmosphere. The preparation method disclosed by the invention adopts an alcohol solvent system and simultaneously gives full stir and ultrasonication, and a ball milling step is arranged in the next drying step, so that the first discharge capacity in an end product can achieve 1537.5 mAh/g, the first efficiency is 95.6%, and the 90% of volume is kept after circulating for 220 times.
Description
Technical field
The invention belongs to the battery manufacture technical field, relate in particular to a kind of preparation method of tin-carbon composite material for cathode of lithium ion battery.
Background technology
Extensive use and fast development along with various portable electric appts and electric automobile, people are also more and more higher to demand and the performance requirement of all kinds of electric product power supplys, lithium rechargeable battery with the superior combination property such as its high power characteristic in success over past ten years and be widely used in the mobile electronic terminal device field.
The specific capacity of graphite negative electrodes material is about 330～350mAh/g at present, can't satisfy people to the demand of high-capacity electrode.The kamash alloy material has caused people's extensive concern with characteristics such as high-energy-density (994mAh/g), high magnification, high securities.But alloy material produces larger volumetric expansion when removal lithium embedded reacts shrinks, electrode material efflorescence easy to crack, and the inner forfeiture of active material electrically contacts, and causes material electrochemical performance to worsen.At present often too complicated about the preparation of tin carbon negative pole material, perhaps raw material too costliness cause cost higher.
Summary of the invention
The object of the invention is to the above-mentioned deficiency for existing lithium ion battery negative material, a kind of preparation method of tin-carbon composite material for cathode of lithium ion battery is provided.
In order to achieve the above object, the present invention has adopted following technical scheme:
The method comprises the steps:
(1) fully be dissolved in synthetic resin in the alcohols solvent;
(2) stir and ultrasonic effect under, at first in the solution of step (1), add pink salt, stir after 3-8 hour, in solution, add graphite, stirred 2-5 hour;
(3) dropwise add ammoniacal liquor in solution, dropping to system pH is 8, and this moment, system was gel;
(4) with system vacuumize under 130-140 ° of C, kept 4-6 hour;
(5) product in the step (4) is carried out mechanical ball milling, then be warming up to 900-1100 ° of C, in atmosphere of inert gases, kept 2-5 hour.
Particularly, the quality share of synthetic resin is 10-25 part, and the quality share of pink salt is 5-20 part, and the quality share of described graphite is 40-75 part; Synthetic resin is phenolic resins or furane resins; Alcohols solvent is n-butanol or normal propyl alcohol; Pink salt is at least a in stannous chloride, butter of tin and the stannic chloride pentahydrate; The quality volume fraction of ammoniacal liquor is 15-25%; In the step (5) inert gas be in nitrogen, helium, neon, argon gas, Krypton and the xenon any or several.
System temperature maintains 50-90 ° of C when preferably, dripping ammoniacal liquor in the step (3); The order number that the middle mechanical ball of step (5) is milled to product is the 80-120 order; Programming rate in the step (5) is 5-15 ° of C/min.
The invention discloses a kind of preparation method of tin-carbon composite material for cathode of lithium ion battery.The method adopts the alcohols solvent system, give simultaneously to stir fully and ultrasonication, so that the tin in the system, graphite and synthetic resin can fully mix, in the step of follow-up drying, be provided with this step of ball milling, reduce particle volume, thereby further guaranteed the cycle performance of product, the first discharge capacity of final products can reach 1537.5mAh/g, efficient 95.6% first, circulates still can keep 90% capacity 220 times.
Embodiment
Below in conjunction with specific embodiments of the invention the technical scheme among the present invention is clearly and completely described.
Embodiment one
The quality share of each raw material among table 1 embodiment one
| Raw material | Phenol-formaldehyde resin | Stannous chloride | Graphite |
| Quality share (part) | 15 | 10 | 50 |
According to the quality share such as listed each component in the table 1,
(1) phenol-formaldehyde resin fully is dissolved in the n-butanol, solution concentration is weight percentage 5%;
(2) stir and ultrasonic effect under, at first in the solution of step (1), add stannous chloride, stir after 3-8 hour, in solution, add graphite, stirred 2-5 hour;
(3) dropwise add the ammoniacal liquor that the quality volume fraction is 15-25% in solution, system temperature maintains 50-90 ° of C, and dropping to system pH is 8, and this moment, system was gel;
(4) with system vacuumize under 130-140 ° of C, kept 4-6 hour;
(5) product in the step (4) is carried out mechanical ball milling, to the order number of product be the 80-120 order, then the programming rate with 5-15 ° of C/min is warming up to 900-1100 ° of C, keeps 2-5 hour in nitrogen atmosphere, obtains product.
Among other embodiment, the phenolic resins in the step (1) can replace with furane resins, and n-butanol can replace with normal propyl alcohol; Stannous chloride in the step (2) can replace with butter of tin or stannic chloride pentahydrate, also can replace with the mixture of stannous chloride, butter of tin and stannic chloride pentahydrate any two or three kinds; Nitrogen in the step (5) can replace with in helium, neon, argon gas, Krypton and the xenon any or appoint several combinations.
Following table is the prescription of other two kinds of tin carbon negative pole materials, and their operating procedure is with embodiment one, shown in the following form of concrete quality share of each component:
The quality share of each raw material among table 2 embodiment two and the embodiment three
| Raw material | Phenol-formaldehyde resin | Stannous chloride | Graphite |
| Embodiment two | 10 | 5 | 40 |
| Embodiment three | 25 | 20 | 75 |
The operating procedure of embodiment two and embodiment three is with embodiment one.
The below is the measured performance parameter of each embodiment:
Each embodiment particular product performance parameters of table 3 is measured
By above-described embodiment as can be known, the tin-carbon composite material for cathode of lithium ion battery for preparing according to the inventive method is at reversible capacity first, all show more outstandingly on efficient and the cycle performance first.
It should be noted that above-described embodiment is not used for limiting claim of the present invention, all other do not break away from the equivalence of finishing under the suggested spirit of the present invention and changes or modification, all should be included in the claim of the present invention.
Claims (10)
1. the preparation method of a tin-carbon composite material for cathode of lithium ion battery is characterized in that: comprise the steps:
(1) fully be dissolved in synthetic resin in the alcohols solvent;
(2) stir and ultrasonic effect under, at first in the solution of step (1), add pink salt, stir after 3-8 hour, in solution, add graphite, stirred 2-5 hour;
(3) dropwise add ammoniacal liquor in solution, dropping to system pH is 8, and this moment, system was gel;
(4) with system vacuumize under 130-140 ° of C, kept 4-6 hour;
(5) product in the step (4) is carried out mechanical ball milling, then be warming up to 900-1100 ° of C, in atmosphere of inert gases, kept 2-5 hour.
2. preparation method according to claim 1, it is characterized in that: the quality share of described synthetic resin is 10-25 part, and the quality share of pink salt is 5-20 part, and the quality share of described graphite is 40-75 part.
3. preparation method according to claim 1, it is characterized in that: described synthetic resin is phenolic resins or furane resins.
4. preparation method according to claim 1, it is characterized in that: described alcohols solvent is n-butanol or normal propyl alcohol.
5. preparation method according to claim 1 is characterized in that: described pink salt is at least a in stannous chloride, butter of tin and the stannic chloride pentahydrate.
6. preparation method according to claim 1, it is characterized in that: the quality volume fraction of described ammoniacal liquor is 15-25%.
7. preparation method according to claim 1 is characterized in that: system temperature maintains 50-90 ° of C when dripping ammoniacal liquor in the described step (3).
8. preparation method according to claim 1 is characterized in that: to be milled to the order number of product be the 80-120 order to mechanical ball in the described step (5).
9. preparation method according to claim 1, it is characterized in that: the programming rate in the described step (5) is 5-15 ° of C/min.
10. preparation method according to claim 1 is characterized in that: in the described step (5) inert gas be in nitrogen, helium, neon, argon gas, Krypton and the xenon any or several.
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| CN2012105049443A CN103050671A (en) | 2012-11-30 | 2012-11-30 | Preparation method of tin carbon composition material for lithium ion battery negative pole |
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| CN2012105049443A CN103050671A (en) | 2012-11-30 | 2012-11-30 | Preparation method of tin carbon composition material for lithium ion battery negative pole |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101017893A (en) * | 2006-02-08 | 2007-08-15 | 深圳市比克电池有限公司 | A tin carbon compound electrode material for lithium ion battery cathode and preparing method |
| CN101740764A (en) * | 2008-11-24 | 2010-06-16 | 上海杉杉科技有限公司 | Tin-graphite composite cathode material for lithium ion battery and preparation method thereof |
| CN102185135A (en) * | 2011-04-13 | 2011-09-14 | 华南理工大学 | Preparation method of tin carbon composite material for negative electrode of lithium ion batteries |
| CN102227019A (en) * | 2011-05-23 | 2011-10-26 | 南京大学 | Method for preparing tin-carbon composite material for cathode of lithium ion battery |
| CN102255079A (en) * | 2011-05-17 | 2011-11-23 | 奇瑞汽车股份有限公司 | Stannum-carbon composite material used for lithium ion battery cathode, preparation method thereof and lithium ion battery |
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- 2012-11-30 CN CN2012105049443A patent/CN103050671A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101017893A (en) * | 2006-02-08 | 2007-08-15 | 深圳市比克电池有限公司 | A tin carbon compound electrode material for lithium ion battery cathode and preparing method |
| CN101740764A (en) * | 2008-11-24 | 2010-06-16 | 上海杉杉科技有限公司 | Tin-graphite composite cathode material for lithium ion battery and preparation method thereof |
| CN102185135A (en) * | 2011-04-13 | 2011-09-14 | 华南理工大学 | Preparation method of tin carbon composite material for negative electrode of lithium ion batteries |
| CN102255079A (en) * | 2011-05-17 | 2011-11-23 | 奇瑞汽车股份有限公司 | Stannum-carbon composite material used for lithium ion battery cathode, preparation method thereof and lithium ion battery |
| CN102227019A (en) * | 2011-05-23 | 2011-10-26 | 南京大学 | Method for preparing tin-carbon composite material for cathode of lithium ion battery |
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Application publication date: 20130417 |